CA1318770C - Methode de fabrication de silice dense tres pure, a grosses particules - Google Patents

Methode de fabrication de silice dense tres pure, a grosses particules

Info

Publication number: CA1318770C
Authority: CA; Canada
Prior art keywords: particle size; silica; high purity; product; micrometers
Prior art date: 1988-04-01
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.): Expired - Fee Related

Application number

CA000593882A

Other languages

English (en)

Inventor

Sheryl A. Robillard

Leo F. Fitzpatrick

Sophia R. Su

Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)

Osram Sylvania Inc

Original Assignee

GTE Products Corp

Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)

1988-04-01

Filing date

1989-03-16

Publication date

1993-06-08

1989-03-16 Application filed by GTE Products Corp filed Critical GTE Products Corp

1993-06-08 Application granted granted Critical

1993-06-08 Publication of CA1318770C publication Critical patent/CA1318770C/fr

2010-06-08 Anticipated expiration legal-status Critical

Status Expired - Fee Related legal-status Critical Current

Links

VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 132
239000002245 particle Substances 0.000 title claims abstract description 60
239000000377 silicon dioxide Substances 0.000 title claims abstract description 59
238000004519 manufacturing process Methods 0.000 title claims abstract description 13
235000012239 silicon dioxide Nutrition 0.000 claims abstract description 31
RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 27
239000000843 powder Substances 0.000 claims abstract description 21
239000002244 precipitate Substances 0.000 claims abstract description 18
VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 11
239000000908 ammonium hydroxide Substances 0.000 claims abstract description 10
238000010438 heat treatment Methods 0.000 claims abstract description 7
LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 36
229960004029 silicic acid Drugs 0.000 claims description 31
239000000047 product Substances 0.000 claims description 21
BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 18
239000002904 solvent Substances 0.000 claims description 7
LRCFXGAMWKDGLA-UHFFFAOYSA-N dioxosilane;hydrate Chemical compound O.O=[Si]=O LRCFXGAMWKDGLA-UHFFFAOYSA-N 0.000 claims description 6
239000000706 filtrate Substances 0.000 claims description 4
238000001914 filtration Methods 0.000 claims description 4
239000004677 Nylon Substances 0.000 claims description 3
238000001354 calcination Methods 0.000 claims description 3
238000001035 drying Methods 0.000 claims description 3
229920001778 nylon Polymers 0.000 claims description 3
230000001590 oxidative effect Effects 0.000 claims description 3
229910052744 lithium Inorganic materials 0.000 claims description 2
229910052700 potassium Inorganic materials 0.000 claims description 2
238000002156 mixing Methods 0.000 claims 2
QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
239000001301 oxygen Substances 0.000 abstract description 3
229910052760 oxygen Inorganic materials 0.000 abstract description 3
230000029087 digestion Effects 0.000 abstract 1
NASVITFAUKYCPM-UHFFFAOYSA-N ethanol;tetraethyl silicate Chemical compound CCO.CCO[Si](OCC)(OCC)OCC NASVITFAUKYCPM-UHFFFAOYSA-N 0.000 abstract 1
238000000034 method Methods 0.000 description 15
229910017974 NH40H Inorganic materials 0.000 description 9
XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
229910001868 water Inorganic materials 0.000 description 8
238000006243 chemical reaction Methods 0.000 description 5
235000011114 ammonium hydroxide Nutrition 0.000 description 4
238000000280 densification Methods 0.000 description 4
239000002585 base Substances 0.000 description 3
230000015572 biosynthetic process Effects 0.000 description 3
229910052681 coesite Inorganic materials 0.000 description 3
229910052906 cristobalite Inorganic materials 0.000 description 3
230000003301 hydrolyzing effect Effects 0.000 description 3
238000006116 polymerization reaction Methods 0.000 description 3
239000011541 reaction mixture Substances 0.000 description 3
229910052710 silicon Inorganic materials 0.000 description 3
239000010703 silicon Substances 0.000 description 3
-1 silicon alkoxides Chemical class 0.000 description 3
229910052682 stishovite Inorganic materials 0.000 description 3
229910052905 tridymite Inorganic materials 0.000 description 3
239000003054 catalyst Substances 0.000 description 2
239000011362 coarse particle Substances 0.000 description 2
239000000084 colloidal system Substances 0.000 description 2
238000009833 condensation Methods 0.000 description 2
230000005494 condensation Effects 0.000 description 2
238000011109 contamination Methods 0.000 description 2
238000000354 decomposition reaction Methods 0.000 description 2
230000000694 effects Effects 0.000 description 2
239000010419 fine particle Substances 0.000 description 2
239000000499 gel Substances 0.000 description 2
125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
239000000203 mixture Substances 0.000 description 2
239000000178 monomer Substances 0.000 description 2
239000002667 nucleating agent Substances 0.000 description 2
238000010899 nucleation Methods 0.000 description 2
230000000704 physical effect Effects 0.000 description 2
238000002360 preparation method Methods 0.000 description 2
239000010453 quartz Substances 0.000 description 2
239000000741 silica gel Substances 0.000 description 2
229910002027 silica gel Inorganic materials 0.000 description 2
229960001866 silicon dioxide Drugs 0.000 description 2
239000007790 solid phase Substances 0.000 description 2
OWNRRUFOJXFKCU-UHFFFAOYSA-N Bromadiolone Chemical compound C=1C=C(C=2C=CC(Br)=CC=2)C=CC=1C(O)CC(C=1C(OC2=CC=CC=C2C=1O)=O)C1=CC=CC=C1 OWNRRUFOJXFKCU-UHFFFAOYSA-N 0.000 description 1
239000004743 Polypropylene Substances 0.000 description 1
229910007156 Si(OH)4 Inorganic materials 0.000 description 1
XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
229910002808 Si–O–Si Inorganic materials 0.000 description 1
239000002253 acid Substances 0.000 description 1
230000002378 acidificating effect Effects 0.000 description 1
230000001476 alcoholic effect Effects 0.000 description 1
239000003513 alkali Substances 0.000 description 1
229910052783 alkali metal Inorganic materials 0.000 description 1
150000001340 alkali metals Chemical class 0.000 description 1
150000001447 alkali salts Chemical class 0.000 description 1
238000000137 annealing Methods 0.000 description 1
239000000919 ceramic Substances 0.000 description 1
239000003153 chemical reaction reagent Substances 0.000 description 1
239000002131 composite material Substances 0.000 description 1
239000013078 crystal Substances 0.000 description 1
230000007547 defect Effects 0.000 description 1
239000008367 deionised water Substances 0.000 description 1
229910021641 deionized water Inorganic materials 0.000 description 1
230000008021 deposition Effects 0.000 description 1
125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
230000008020 evaporation Effects 0.000 description 1
238000001704 evaporation Methods 0.000 description 1
239000005350 fused silica glass Substances 0.000 description 1
239000007789 gas Substances 0.000 description 1
239000011521 glass Substances 0.000 description 1
230000007062 hydrolysis Effects 0.000 description 1
238000006460 hydrolysis reaction Methods 0.000 description 1
239000012535 impurity Substances 0.000 description 1
230000001788 irregular Effects 0.000 description 1
238000012986 modification Methods 0.000 description 1
230000004048 modification Effects 0.000 description 1
VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 1
230000000877 morphologic effect Effects 0.000 description 1
230000006911 nucleation Effects 0.000 description 1
238000012856 packing Methods 0.000 description 1
239000012071 phase Substances 0.000 description 1
229920001155 polypropylene Polymers 0.000 description 1
238000003825 pressing Methods 0.000 description 1
239000011164 primary particle Substances 0.000 description 1
239000004576 sand Substances 0.000 description 1
150000004760 silicates Chemical class 0.000 description 1
125000005624 silicic acid group Chemical group 0.000 description 1
239000003381 stabilizer Substances 0.000 description 1
239000000725 suspension Substances 0.000 description 1
238000003786 synthesis reaction Methods 0.000 description 1
230000002194 synthesizing effect Effects 0.000 description 1
LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1

Classifications

- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/16—Preparation of silica xerogels
- C01B33/163—Preparation of silica xerogels by hydrolysis of organosilicon compounds, e.g. ethyl orthosilicate
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/02—Amorphous compounds
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/11—Powder tap density
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content

Landscapes

Chemical & Material Sciences (AREA)
Organic Chemistry (AREA)
Inorganic Chemistry (AREA)
Dispersion Chemistry (AREA)
Life Sciences & Earth Sciences (AREA)
Engineering & Computer Science (AREA)
Chemical Kinetics & Catalysis (AREA)
General Chemical & Material Sciences (AREA)
Geochemistry & Mineralogy (AREA)
Materials Engineering (AREA)
Silicon Compounds (AREA)

CA000593882A 1988-04-01 1989-03-16 Methode de fabrication de silice dense tres pure, a grosses particules Expired - Fee Related CA1318770C (fr)

Applications Claiming Priority (2)

Application Number	Priority Date	Filing Date	Title
US07/176,582 US4940571A (en)	1988-04-01	1988-04-01	Method of making large particle size, high purity dense silica
US176,582		1988-04-01

Publications (1)

Publication Number	Publication Date
CA1318770C true CA1318770C (fr)	1993-06-08

Family

ID=22644945

Family Applications (1)

Application Number	Title	Priority Date	Filing Date
CA000593882A Expired - Fee Related CA1318770C (fr)	1988-04-01	1989-03-16	Methode de fabrication de silice dense tres pure, a grosses particules

Country Status (6)

Country	Link
US (1)	US4940571A (fr)
EP (1)	EP0335175B1 (fr)
JP (1)	JPH01290522A (fr)
KR (1)	KR890015957A (fr)
CA (1)	CA1318770C (fr)
DE (1)	DE68908223T2 (fr)

Families Citing this family (17)

* Cited by examiner, † Cited by third party
Publication number	Priority date	Publication date	Assignee	Title
DE69227448T2 (de) *	1992-06-19	1999-07-01	Cu Chemie Uetikon Ag, Uetikon	Verfahren zur Herstellung von Pulvern und Suspensionen von amorphen Siliziumdioxidmikrokugeln
US5425930A (en) *	1993-09-17	1995-06-20	Alliedsignal Inc.	Process for forming large silica spheres by low temperature nucleation
US6156285A (en) *	1998-11-12	2000-12-05	Dow Corning Corporation	Method for densifying particulate silica
KR100329123B1 (ko) *	1999-08-28	2002-03-21	윤덕용	웨이퍼 폴리싱용 실리카 슬러리의 제조 방법
US9249028B2 (en)	2010-02-08	2016-02-02	Momentive Performance Materials Inc.	Method for making high purity metal oxide particles and materials made thereof
US8197782B2 (en) *	2010-02-08	2012-06-12	Momentive Performance Materials	Method for making high purity metal oxide particles and materials made thereof
US9561473B2 (en)	2014-02-28	2017-02-07	Pall Corporation	Charged hollow fiber membrane having hexagonal voids
US9764292B2 (en)	2014-02-28	2017-09-19	Pall Corporation	Porous polymeric membrane with high void volume
US9309126B2 (en)	2014-02-28	2016-04-12	Pall Corporation	Rapidly dissolvable nanoparticles
US9610548B2 (en)	2014-02-28	2017-04-04	Pall Corporation	Composite porous polymeric membrane with high void volume
US9446355B2 (en)	2014-02-28	2016-09-20	Pall Corporation	Porous polymeric membrane with high void volume
US9776142B2 (en)	2014-02-28	2017-10-03	Pall Corporation	Porous polymeric membrane with high void volume
US9737860B2 (en)	2014-02-28	2017-08-22	Pall Corporation	Hollow fiber membrane having hexagonal voids
US9302228B2 (en)	2014-02-28	2016-04-05	Pall Corporation	Charged porous polymeric membrane with high void volume
US9970869B2 (en)	2015-07-24	2018-05-15	Chevron Phillips Chemical Company Lp	Use of turbidimeter for measurement of solid catalyst system component in a reactor feed
EP3543212A4 (fr) *	2016-11-16	2019-12-04	Mitsubishi Chemical Corporation	Poudre de silice pour alimentation quantitative, kit de purification pour matériau biologique l'utilisant, et sa méthode de production
US11345606B2 (en) *	2017-02-17	2022-05-31	David Brown	Deposition particles and a method and apparatus for producing the same

Family Cites Families (16)

* Cited by examiner, † Cited by third party
Publication number	Priority date	Publication date	Assignee	Title
US2974105A (en) *	1956-05-01	1961-03-07	Du Pont	Silica organosols and their preparation
US3311481A (en) *	1962-03-01	1967-03-28	Hitco	Refractory fibers and methods of making them
US3538015A (en) *	1967-12-07	1970-11-03	Nalco Chemical Co	Large particle silica sols and method of production
US4246139A (en) *	1975-09-15	1981-01-20	Phillips Petroleum Company	Silica production
US4059658A (en) *	1975-09-15	1977-11-22	Corning Glass Works	Low temperature production of high purity fused silica
GR66589B (fr) *	1978-06-22	1981-03-30	Snam Progetti
SU865791A1 (ru) *	1978-08-11	1981-09-23	Ордена Ленина Институт Общей И Неорганический Химии Им. Н.С.Курнакова Ан Ссср	Способ получени сферического силикагел
SE422045C (sv) *	1979-04-30	1985-03-18	Guy Von Dardel	Sett att framstella silikaaerogel i form av ett vesentligen sprickfritt, foretredesvis transparent block samt anvendning av detsamma i solpaneler
US4339559A (en) *	1980-05-21	1982-07-13	Phillips Petroleum Company	Polymerization using silica from single phase controlled hydrolysis of silicate ester
CA1172045A (fr) *	1980-09-16	1984-08-07	Shiro Kurosaki	Methode de production d'un verre d'optique
FR2507171A1 (fr) *	1981-06-04	1982-12-10	Zarzycki Jerzy	Aerogels de silice monolithiques, leur preparation et leur utilisation pour la preparation d'articles en verre de silice et de materiaux thermiquement isolants
US4426216A (en) *	1982-01-06	1984-01-17	Hitachi, Ltd.	Process for producing optical glass
US4574063A (en) *	1983-05-09	1986-03-04	Corning Glass Works	Method of forming glass or ceramic article
US4560399A (en) *	1984-10-22	1985-12-24	Corning Glass Works	Method for making glass or ceramic article
US4680049A (en) *	1986-08-15	1987-07-14	Gte Laboratories Incorporated	Process for molding optical components of silicate glass to a near net shape optical precision
US4788046A (en) *	1987-08-13	1988-11-29	Ceramics Process Systems Corporation	Method for producing materials for co-sintering

1988
- 1988-04-01 US US07/176,582 patent/US4940571A/en not_active Expired - Fee Related
1989
- 1989-03-15 EP EP89104604A patent/EP0335175B1/fr not_active Expired - Lifetime
- 1989-03-15 DE DE89104604T patent/DE68908223T2/de not_active Expired - Fee Related
- 1989-03-16 CA CA000593882A patent/CA1318770C/fr not_active Expired - Fee Related
- 1989-03-31 JP JP1078716A patent/JPH01290522A/ja active Pending
- 1989-04-01 KR KR1019890004303A patent/KR890015957A/ko not_active Withdrawn

Also Published As

Publication number	Publication date
DE68908223T2 (de)	1993-11-25
JPH01290522A (ja)	1989-11-22
EP0335175A3 (fr)	1991-09-18
EP0335175B1 (fr)	1993-08-11
EP0335175A2 (fr)	1989-10-04
DE68908223D1 (de)	1993-09-16
US4940571A (en)	1990-07-10
KR890015957A (ko)	1989-11-27

Legal Events

Date	Code	Title	Description
1995-12-10	MKLA	Lapsed

Publication	Publication Date	Title
CA1318770C (fr)	1993-06-08	Methode de fabrication de silice dense tres pure, a grosses particules
Hatakeyama et al.	1990	Synthesis of monodispersed spherical β‐silicon carbide powder by a sol‐gel process
US5989510A (en)	1999-11-23	Method of producing granular amorphous silica
JPS62275022A (ja)	1987-11-30	新規な形態学的特徴を有する酸化第二セリウム
KR102070380B1 (ko)	2020-01-29	합성-헥토라이트의 저온 상압 제조방법
USH626H (en)	1989-04-04	Sol-gel ceramic oxides
JP2000247625A (ja)	2000-09-12	高純度シリカゾル及びその製造方法
CA1318481C (fr)	1993-06-01	Methode de fabrication de silice dense tres pure a grosses particules
JPH10512231A (ja)	1998-11-24	メソ多孔性結晶性物質の調製方法
US4226636A (en)	1980-10-07	Production of calcium silicate having high specific bulk volume and calcium silicate-gypsum composite
KR101595792B1 (ko)	2016-02-22	졸겔법에 의한 크기-제어된 실리카-지르코니아 복합졸의 제조방법
CN113620303B (zh)	2022-11-29	一种中性条件下制备多孔纳米二氧化硅小球的方法
CN112374504B (zh)	2023-01-24	一种物理法制造纳米二氧化硅的工艺
US4774068A (en)	1988-09-27	Method for production of mullite of high purity
JP2827616B2 (ja)	1998-11-25	封止材用錫酸亜鉛粉末およびその製造方法と用途
JPS6045125B2 (ja)	1985-10-08	アルミナゾルの製造法
Tsurita et al.	1997	Preparation of SiO2-ZrO2-Na2O Porous Glass Supports.
CA2398876A1 (fr)	2001-07-26	Procede sol-gel permettant de produire un verre de silice synthetique
KR950013368B1 (ko)	1995-11-02	알루미노실리케이트-기재의 안료, 그 제조방법 및 충전물로의 그 용도
JP2607118B2 (ja)	1997-05-07	球状有機珪酸および球状シリカ粉末の製造法
JP5483814B2 (ja)	2014-05-07	コロイド状フォージャサイト型ゼオライトおよびその合成方法
JP3260143B2 (ja)	2002-02-25	結晶性層状珪酸およびその製造方法
JPH0825740B2 (ja)	1996-03-13	均一粒子径、高結晶度、高純度合成カオリナイト及びその製造方法
JP2838802B2 (ja)	1998-12-16	ジルコン粉末の合成法
KR101025567B1 (ko)	2011-03-28	지오폴리머를 이용한 윌레마이트의 제조방법